CN112768835A - Cr (chromium)3AlC2Preparation method of/PVDF-PVA lithium ion battery diaphragm - Google Patents
Cr (chromium)3AlC2Preparation method of/PVDF-PVA lithium ion battery diaphragm Download PDFInfo
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to Cr3AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm comprises the following raw materials: chromium powder, aluminum powder, graphite powder, chromium carbide, polyvinylidene fluoride, polyvinyl alcohol and N, N-diMethyl formamide; the preparation method comprises the following steps: firstly, calcining chromium powder, aluminum powder and graphite powder at high temperature to obtain Cr2AlC followed by Cr2Calcining AlC at high temperature in chromium carbide to obtain Cr2AlC2Then loading the mixed solution into PVDF-PVA mixed solution, coating the mixed solution on a glass plate, and drying the glass plate to obtain Cr3AlC2The prepared PVDF-PVA film is used for the lithium ion battery diaphragm and has stronger mechanical strength, larger porosity and good charge-discharge cycle performance.
Description
Technical Field
The invention relates to the field of diaphragms, in particular to Cr3AlC2A preparation method of a PVDF-PVA lithium ion battery diaphragm.
Background
Lithium ion batteries have many advantages such as high energy density, large output power, and good cycle stability, and have gradually replaced conventional secondary batteries, which are called as new secondary batteries. The lithium ion battery is widely applied to 3C products, such as digital cameras, mobile phones, notebook computers, electric bicycles and the like, and also covers the large industrial fields of electric automobiles, energy storage power stations, military equipment, aerospace and the like. The main components of the lithium ion battery are a positive electrode, a negative electrode and a diaphragm. The lithium battery diaphragm is one of the key inner layer components in the structure of the lithium ion battery, the performance of the lithium battery diaphragm determines the properties of the battery, such as interface structure, internal resistance and the like, and directly influences the properties of the battery, such as capacity, cycle, safety performance and the like. The most important lithium ion battery separator in the market is an olefin-based separator, olefin has good thermal stability, but the mechanical strength of olefin is low, so that the development of a separator with high stability and good mechanical strength is a current research hotspot.
At present, the mechanical property of the diaphragm is mainly improved by adding ceramic inorganic materials into the diaphragm, and although the mechanical property of the diaphragm can be improved by adding the inorganic materials, the battery performance of the diaphragm is affected due to the fact that the inorganic materials are generally weak in conductivity.
Disclosure of Invention
The invention provides Cr3AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm comprises the following steps:
s1: putting chromium powder, aluminum powder and graphite powder into a ball mill, stirring and mixing for 6-10h, then sieving the mixed raw materials with a 60-80 mesh sieve, filling into a die, and pressing into a blank;
s2: quickly loading the blank into a crucible, putting the crucible into a vacuum sintering furnace, carrying out calcination reaction under the protection of argon, and cooling to obtain Cr2AlC powder;
s3: cr obtained in S22Placing AlC powder and CrC powder into a ball mill, stirring and mixing, pressing into a blank, quickly placing into a crucible, placing into a vacuum sintering furnace, pressurizing to 20-30kPa, carrying out calcination reaction under the protection of argon, and cooling to obtain Cr3AlC2Powder;
s4: adding polyvinylidene fluoride into N, N-dimethylformamide, stirring at 60 deg.C for 30-60min, dissolving polyvinyl alcohol in deionized water, mixing the two solutions, stirring for 20-30min, and adding S3 product Cr3AlC2Stirring the powder for 30-60min to mix uniformly;
s5: uniformly coating the S4 mixed solution on a clean and flat glass plate, then transferring the glass plate into a drying box for drying, and cooling to room temperature to obtain Cr3AlC2The PVDF-PVA lithium ion battery diaphragm.
Preferably, in step S1, the molar ratio of the chromium powder, the aluminum powder, and the graphite powder is 2: 1: 1.
preferably, in the step S2, the calcination temperature is 1400-1500 ℃, and the calcination time is 3-4 h.
Preferably, in the step S3, the molar ratio of the chromium powder to the CrC powder is 2: 1.
Preferably, in the step S3, the calcination temperature is 1200-1300 ℃, and the calcination time is 4-6 h.
Preferably, in step S4, the mass-to-volume ratio of the polyvinylidene fluoride to the polyvinyl alcohol to the N, N-dimethylformamide is 1 g: (0.5-0.6) g: (5-10) ml.
Preferably, in the step S5, the drying temperature is 100-120 ℃, and the drying time is 8-10 h.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention synthesizes Cr by using chromium powder, aluminum powder and graphite powder at high temperature2AlC powder, using Cr2High-temperature reaction of AlC powder and CrC powder to obtain Cr3AlC2Powder, simple process, and Cr obtained3AlC2The purity of the powder is high.
(2) The invention is prepared by mixing Cr3AlC2The powder is loaded on the PVDF and PVA mixed membrane, so that the mechanical strength and the porosity of the membrane are improved.
(3)Cr3AlC2As a conductive ceramic, has good conductivity by adding Cr3AlC2Powder loadingOn the diaphragm, the mechanical strength of the diaphragm is improved, and the conductivity of the diaphragm is improved, so that the diaphragm has better charge-discharge cycle performance when used as a battery.
(4) The raw materials used in the invention have wide sources, and the preparation method is simple and is suitable for large-scale production.
Drawings
FIG. 1 is a graph showing the charge and discharge cycle characteristics of thin films prepared in examples 1 to 4 of the present invention and comparative example 1 when they are used as battery separators.
Detailed Description
Example 1:
cr (chromium)3AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm comprises the following steps:
s1: putting 40mmol of chromium powder, 20mmol of aluminum powder and 20mmol of graphite powder into a ball mill, stirring and mixing for 8 hours, then sieving the mixed raw materials with a 80-mesh sieve, then putting into a die, and pressing into a blank;
s2: quickly loading the blank into a crucible, putting the crucible into a vacuum sintering furnace, calcining the blank at 1450 ℃ for 3.5h under the protection of argon, and cooling to obtain Cr2AlC powder;
s3: cr obtained in S22Placing AlC powder and 20mmol CrC powder into a ball mill, stirring and mixing at the rotating speed of 30rpm/min, then pressing into a blank, quickly placing into a crucible, placing into a vacuum sintering furnace, pressurizing to 25kPa, calcining at 1250 ℃ for 5h under the protection of argon, and cooling to obtain Cr3AlC2Powder;
s4: adding 2g of polyvinylidene fluoride into 15ml of N, N-dimethylformamide, stirring for 45min, adding 1.1g of polyvinyl alcohol into 20nl of deionized water, mixing the two solutions, continuing stirring for 25min, and adding S3 product Cr3AlC2Stirring the powder for 45min to mix uniformly;
s5: uniformly coating the S4 mixed solution on a clean and flat glass plate, then transferring the glass plate into a drying oven, drying for 9h at 140 ℃, and cooling to room temperature to obtain Cr3AlC2The PVDF-PVA lithium ion battery diaphragm.
Example 2:
cr (chromium)3AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm comprises the following steps:
s1: putting 40mmol of chromium powder, 20m of aluminum powder and 20mmol of graphite powder into a ball mill, stirring and mixing for 6 hours, then sieving the mixed raw materials with a 60-mesh sieve, filling into a die, and pressing into a blank;
s2: quickly loading the blank into a crucible, putting the crucible into a vacuum sintering furnace, calcining for 4 hours at 1400 ℃ under the protection of argon, and cooling to obtain Cr2AlC powder;
s3: cr obtained in S22Placing AlC powder and 20mmol CrC powder into a ball mill, stirring and mixing, pressing into a blank, rapidly placing into a crucible, placing into a vacuum sintering furnace, pressurizing to 20kPa, calcining at 1200 ℃ for 6h under the protection of argon, and cooling to obtain Cr3AlC2Powder;
s4: adding 2g of polyvinylidene fluoride into 10ml of N, N-dimethylformamide, stirring for 30min, adding 1g of polyvinyl alcohol into 20ml of deionized water, mixing the two solutions, continuously stirring for 20min, and adding S3 product Cr3AlC2Stirring the powder for 30min to mix uniformly;
s5: uniformly coating the S4 mixed solution on a clean and flat glass plate, then transferring the glass plate into a drying oven for drying, drying for 10h at 120 ℃, and cooling to room temperature to obtain Cr3AlC2The PVDF-PVA lithium ion battery diaphragm.
Example 3:
cr (chromium)3AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm comprises the following steps:
s1: putting 40mmol of chromium powder, 20mmol of aluminum powder and 20mmol of graphite powder into a ball mill, stirring and mixing for 10 hours, then sieving the mixed raw materials by a 60-mesh sieve, then putting into a die, and pressing into a blank;
s2: quickly loading the blank into a crucible, putting the crucible into a vacuum sintering furnace, calcining for 3h at 1500 ℃ under the protection of argon, and cooling to obtain Cr2AlC powder;
s3: cr obtained in S22Placing AlC powder and 20mmol CrC powder into a ball mill, stirring and mixing, and pressing into a blankQuickly putting the mixture into a crucible, putting the crucible into a vacuum sintering furnace, pressurizing to 30kPa, calcining for 4h at 1300 ℃ under the protection of argon, and cooling to obtain Cr3AlC2Powder;
s4: adding 2g of polyvinylidene fluoride into 20ml of N, N-dimethylformamide, stirring for 60min, adding 1.2g of polyvinyl alcohol into 20ml of deionized water, mixing the two solutions, continuing stirring for 30min, and adding S3 product Cr3AlC2Stirring the powder for 60min to mix uniformly;
s5: uniformly coating the S4 mixed solution on a clean and flat glass plate, then transferring the glass plate into a drying oven for drying, drying for 8h at 150 ℃, and cooling to room temperature to obtain Cr3AlC2The PVDF-PVA lithium ion battery diaphragm.
Example 4:
cr (chromium)3AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm comprises the following steps:
s1: putting 40mmol of chromium powder, 20mmol of aluminum powder and 20mmol of graphite powder into a ball mill, stirring and mixing for 8 hours, then sieving the mixed raw materials with a 80-mesh sieve, then putting into a die, and pressing into a blank;
s2: quickly loading the blank into a crucible, putting the crucible into a vacuum sintering furnace, calcining the blank for 3.2 hours at 1420 ℃ in the argon protective atmosphere, and cooling to obtain Cr2AlC powder;
s3: cr obtained in S22Placing AlC powder and 20mmol CrC powder into a ball mill, stirring and mixing at the rotating speed of 30rpm/min, then pressing the mixture into a blank, quickly placing the blank into a crucible, placing the crucible into a vacuum sintering furnace, pressurizing to 25kPa, calcining for 5 hours at 1250 ℃ under the protection of argon gas, and cooling to obtain Cr3AlC2Powder;
s4: adding 2g of polyvinylidene fluoride into 15ml of N, N-dimethylformamide, stirring for 45min, adding 1.1g of polyvinyl alcohol into 20ml of deionized water, mixing the two solutions, continuing stirring for 25min, and adding S3 product Cr3AlC2Stirring the powder for 40min to mix uniformly;
s5: uniformly coating the S4 mixed solution on a clean and flat glass plate, and then coating the glass plate with the S4 mixed solutionIt is transferred into a drying oven, dried for 9h at 140 ℃, cooled to room temperature to obtain Cr3AlC2The PVDF-PVA lithium ion battery diaphragm.
Comparative example 1:
without addition of Cr3AlC2The preparation method of the PVDF-PVA diaphragm comprises the following steps:
s1: adding 2g of polyvinylidene fluoride into 15ml of N, N-dimethylformamide, stirring for 45min, adding 1.1g of polyvinyl alcohol, and continuing stirring for 25 min;
s2: uniformly coating the S1 mixed solution on a clean and flat glass plate, then transferring the glass plate into a drying oven, drying for 9h at 140 ℃, and cooling to room temperature to obtain Cr3AlC2The PVDF-PVA lithium ion battery diaphragm.
And (3) performance testing:
the tensile strength and the puncture strength of the separator obtained in examples 1 to 4 and the separator obtained in comparative example 1 were measured.
Testing method of puncture strength of the diaphragm: the puncture strength of the membrane was measured using a puncture instrument, specifically using a 1mm diameter needle with no sharp edge at the tip, piercing the membrane vertically at a speed of 2m/min, and recording the data using a FGN-5B data recorder, with the experimental results as shown in table 1.
Tensile strength was tested according to the national standard GB/T1040.3-2008 for examples 1-4 and comparative example 1, with properties given in Table 1.
And (3) porosity testing:
the dried separators prepared in examples 1 to 4 and comparative example 1 were used to prepare 15 mm. times.15 mm-sized samples and their mass was weighed and recorded as m0And meanwhile, measuring the thickness d by a micrometer screw gauge, then putting the obtained product into n-butyl alcohol, soaking for 2 hours, adsorbing excessive n-butyl alcohol on the surface, and weighing again. The porosity (ψ) is calculated as follows:
in the formula m0For the membrane mass before infiltration, m1For the quality of the separator after soaking in n-butanol, V0Is prepared by soakingThe volume of the separator before moistening, rho is the density of n-butanol, and the density of n-butanol relative to water is 0.81 g/ml. The test results are shown in Table 1.
Assembling a button type simulation battery in a glove box filled with argon by adopting LiCoO2The material is a positive electrode, graphite is a negative electrode, the materials prepared in examples 1-4 and comparative example 1 are diaphragms, and electrolyte is dripped into a glove box to form the button cell. The button cell is formed in the sleeve box. The stacking sequence when assembling the battery is positive shell, shrapnel, gasket, positive plate, diaphragm, electrolyte, negative pole, gasket and negative shell. And standing the assembled button cell for 12h, and performing charge-discharge cycle test on the button cell by using a NEWARE cell test system. The discharge capacity retention rate was calculated by the following formula:
as shown in FIG. 1, the separators prepared in examples 1 to 4 had higher specific discharge capacities than the separator prepared in comparative example 1, wherein the specific discharge capacity before cycling of the separator prepared in example 1 was 162.3mA h g-1And the specific discharge capacity after 600 cycles is 153.6mAh g-1The capacity retention rate reached 94.6%, and the specific discharge capacity of the separators prepared in examples 2 to 4 after 600 cycles was also higher than 140mAh g-1The capacity retention rate is higher than 85%, and the specific discharge capacity of the diaphragm circulating ring prepared in comparative example 1 is 121.5mAh g-178.32mAh g after 600 cycles-1The capacity retention rate was 63.3%, demonstrating Cr3AlC2The load of (b) improves the charge-discharge cycle performance of the separator when used as a battery.
Table 1: mechanical Strength and porosity Performance data for examples 1-4 and comparative example 1
As can be seen from Table 1, the tensile strength, septum puncture strength and porosity of the films prepared in examples 1-4 are all higher than those of the films prepared in examplesThe film prepared in comparative example 1, which demonstrated Cr3AlC2The load of (b) increases the mechanical strength and porosity of the separator.
Claims (7)
1. Cr (chromium)3AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm is characterized by comprising the following steps:
s1: putting chromium powder, aluminum powder and graphite powder into a ball mill, stirring and mixing for 6-10h, then sieving the mixed raw materials with a 60-80 mesh sieve, filling into a die, and pressing into a blank;
s2: quickly loading the blank into a crucible, putting the crucible into a vacuum sintering furnace, carrying out calcination reaction under the protection of argon, and cooling to obtain Cr2AlC powder;
s3: cr obtained in S22Placing AlC powder and CrC powder into a ball mill, stirring and mixing, pressing into a blank, quickly placing into a crucible, placing into a vacuum sintering furnace, pressurizing to 20-30kPa, carrying out calcination reaction under the protection of argon, and cooling to obtain Cr3AlC2Powder;
s4: adding polyvinylidene fluoride into N, N-dimethylformamide, stirring at 60 deg.C for 30-60min, dissolving polyvinyl alcohol in deionized water, mixing the two solutions, stirring for 20-30min, and adding S3 product Cr3AlC2Stirring the powder for 30-60min to mix uniformly;
s5: uniformly coating the S4 mixed solution on a clean and flat glass plate, then transferring the glass plate into a drying box for drying, and cooling to room temperature to obtain Cr3AlC2The PVDF-PVA lithium ion battery diaphragm.
2. The Cr of claim 13AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm is characterized in that in the step S1, the molar ratio of the chromium powder, the aluminum powder and the graphite powder is 2: 1: 1.
3. the Cr of claim 13AlC2The preparation method of the PVDF-PVA lithium ion battery diaphragm is characterized in thatIn the step S2, the calcination temperature is 1400-1500 ℃, and the calcination time is 3-4 h.
4. The Cr of claim 13AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm is characterized in that in the step S3, the molar ratio of the chromium powder to the CrC powder is 2: 1.
5. The Cr of claim 13AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm is characterized in that in the step S3, the calcination temperature is 1200-1300 ℃, and the calcination time is 4-6 h.
6. The Cr of claim 13AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm is characterized in that in the step S4, the mass-volume ratio of the polyvinylidene fluoride to the polyvinyl alcohol to the N, N-dimethylformamide is 1 g: (0.5-0.6) g: (5-10) ml.
7. The Cr of claim 13AlC2The preparation method of the/PVDF-PVA lithium ion battery diaphragm is characterized in that in the step S5, the drying temperature is 100-120 ℃, and the drying time is 8-10 h.
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